Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768103011509/br0115sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768103011509/br01151Xsup2.rtv | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768103011509/br01152Xsup3.rtv | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768103011509/br01153Nsup4.rtv | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768103011509/br0115sup5.pdf |
Pb5Al3F19 | V = 1473.39 (4) Å3 |
Mr = 1477.94 | Z = 4 |
Triclinic, I1 | F(000) = 2480 |
Hall symbol: -I 1 | Dx = 6.663 (1) Mg m−3 Dm = 6.66 (5) Mg m−3 Dm measured by phase IV, by immersion in bromobenzene |
a = 14.2624 (2) Å | ? radiation, λ = ? Å |
b = 14.2808 (2) Å | T = 320 K |
c = 7.2340 (1) Å | Particle morphology: plate like |
α = 90.001 (10)° | colourless |
β = 90.509 (1)° | ?, ? × ? × ? mm |
γ = 90.001 (10)° |
Refinement on Inet | 146 parameters |
Least-squares matrix: full with fixed elements per cycle | 0 restraints |
Rp = 0.078 | 0 constraints |
Rwp = 0.112 | Weighting scheme based on measured s.u.'s |
Rexp = 0.049 | (Δ/σ)max = 0.05 |
χ2 = 5.290 | Background function: Polynomial of order 5 for each dataset. |
? data points | Preferred orientation correction: none |
Profile function: pseudo-Voigt |
Pb5Al3F19 | β = 90.509 (1)° |
Mr = 1477.94 | γ = 90.001 (10)° |
Triclinic, I1 | V = 1473.39 (4) Å3 |
a = 14.2624 (2) Å | Z = 4 |
b = 14.2808 (2) Å | ? radiation, λ = ? Å |
c = 7.2340 (1) Å | T = 320 K |
α = 90.001 (10)° | ?, ? × ? × ? mm |
Experimental. Pb5 Al3 F19 melts incongruently at 825 (5) K, the thermal limit of crystalline stability. |
Geometry. atomic displacements at the phase transition from phase III to phase II are < or = 0.33 Å by Pb, < or = 0.37 Å by Al and < or = 0.69 Å by F; at the phase transition to phase IV, the atomic displacements are < or = 0.53 Å by Pb, < or 0.49 Å by Al and < or = 0.92 Å by F. |
Refinement. Simultaneous refinement of dataset 1, dataset 2 and dataset 3 |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.2603 (2) | 0.4174 (2) | 0.5038 (6) | 0.030 (1)* | |
Pb2 | 0.4124 (5) | −0.2633 (5) | 0.4920 (3) | 0.027 (2)* | |
Pb3 | 0.2222 (3) | −0.0623 (3) | 0.4967 (7) | 0.034 (2)* | |
Pb4 | 0.0610 (3) | 0.2110 (3) | 0.5001 (5) | 0.025 (5)* | |
Pb5 | 0.0023 (5) | 0.4772 (2) | 0.2557 (14) | 0.052 (1)* | |
Al1 | 0.1519 (14) | 0.3193 (13) | −0.010 (3) | 0.007 (1)* | |
Al2 | 0.6925 (13) | 0.1735 (13) | 0.021 (3) | 0.007 (1)* | |
Al3 | 0.0044 (17) | 0.0128 (13) | 0.245 (3) | 0.007 (1)* | |
F1 | 0.2878 (13) | 0.1155 (13) | 0.681 (3) | 0.027 (1)* | |
F2 | 0.6116 (16) | −0.2637 (17) | 0.339 (3) | 0.027 (1)* | |
F3 | 0.2606 (14) | 0.6116 (14) | 0.349 (3) | 0.012 (1)* | |
F4 | −0.2519 (14) | 0.3867 (15) | 0.333 (2) | 0.012 (1)* | |
F5 | 0.5735 (13) | 0.2107 (13) | 0.149 (2) | 0.012 (1)* | |
F6 | 0.4092 (12) | 0.2165 (15) | 0.305 (3) | 0.027 (1)* | |
F7 | 0.1895 (13) | 0.4066 (14) | 0.175 (3) | 0.027 (1)* | |
F8 | −0.0912 (11) | 0.2937 (13) | 0.687 (3) | 0.012 (1)* | |
F9 | 0.0391 (13) | 0.3871 (14) | −0.045 (2) | 0.027 (1)* | |
F10 | 0.6078 (11) | 0.0683 (10) | −0.007 (3) | 0.012 (1)* | |
F11 | 0.2524 (15) | 0.2458 (13) | 0.055 (2) | 0.027 (1)* | |
F12 | 0.7357 (10) | 0.2641 (11) | 0.015 (3) | 0.012 (1)* | |
F13 | 0.00000 | 0.00000 | 0.50000 | 0.039 (2)* | |
F14 | 0.00000 | 0.00000 | 0.00000 | 0.039 (2)* | |
F15 | 0.1171 (14) | 0.0421 (14) | 0.254 (3) | 0.025 (1)* | |
F16 | −0.1273 (14) | −0.0583 (14) | 0.270 (3) | 0.025 (1)* | |
F17 | −0.0565 (15) | 0.1069 (16) | 0.711 (3) | 0.025 (1)* | |
F18 | 0.0588 (14) | −0.1055 (15) | 0.740 (3) | 0.025 (1)* | |
F19 | 0.1284 (15) | 0.5927 (14) | 0.037 (2) | 0.024 (1)* | |
F20 | 0.5811 (13) | −0.1257 (13) | 0.005 (3) | 0.024 (1)* |
Al1—F1i | 1.78 (3) | Al2—F8i | 2.12 (4) |
Al1—F2ii | 1.71 (4) | Al2—F10 | 1.94 (3) |
Al1—F6i | 1.80 (3) | Al2—F12 | 1.43 (3) |
Al1—F7 | 1.90 (3) | Al3—F13 | 1.85 (3) |
Al1—F9 | 1.87 (4) | Al3—F14 | 1.78 (3) |
Al1—F11 | 1.83 (4) | Al3—F15 | 1.66 (4) |
Al2—F3iii | 1.81 (4) | Al3—F16 | 2.14 (4) |
Al2—F4i | 1.60 (4) | Al3—F17iv | 1.89 (4) |
Al2—F5 | 2.01 (4) | Al3—F18iv | 1.61 (4) |
F1i—Al1—F2ii | 95 (1) | F4i—Al2—F12 | 106 (1) |
F1i—Al1—F6i | 164 (3) | F5—Al2—F8i | 72 (1) |
F1i—Al1—F7 | 91 (1) | F5—Al2—F10 | 74 (1) |
F1i—Al1—F9 | 94 (1) | F5—Al2—F12 | 98 (2) |
F1i—Al1—F11 | 95 (1) | F8i—Al2—F10 | 71 (1) |
F2ii—Al1—F6i | 99 (1) | F8i—Al2—F12 | 94 (1) |
F2ii—Al1—F7 | 175 (4) | F10—Al2—F12 | 165 (2) |
F2ii—Al1—F9 | 88 (1) | F13—Al3—F14 | 168 (2) |
F2ii—Al1—F11 | 91 (2) | F13—Al3—F15 | 92 (1) |
F6i—Al1—F7 | 75 (1) | F13—Al3—F16 | 81 (1) |
F6i—Al1—F9 | 80 (1) | F13—Al3—F17iv | 76 (1) |
F6i—Al1—F11 | 91 (1) | F13—Al3—F18iv | 89 (1) |
F7—Al1—F9 | 90 (1) | F14—Al3—F15 | 95 (1) |
F7—Al1—F11 | 89 (1) | F14—Al3—F16 | 91 (1) |
F9—Al1—F11 | 171 (2) | F14—Al3—F17iv | 95 (1) |
F3iii—Al2—F4i | 85 (1) | F14—Al3—F18iv | 98 (1) |
F3iii—Al2—F5 | 155 (2) | F15—Al3—F16 | 165 (2) |
F3iii—Al2—F8i | 89 (1) | F15—Al3—F17iv | 81 (1) |
F3iii—Al2—F10 | 84 (1) | F15—Al3—F18iv | 110 (1) |
F3iii—Al2—F12 | 101 (1) | F16—Al3—F17iv | 84 (1) |
F4i—Al2—F5 | 106 (2) | F16—Al3—F18iv | 84 (1) |
F4i—Al2—F8i | 165 (9) | F17iv—Al3—F18iv | 163 (2) |
F4i—Al2—F10 | 89 (1) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1/2; (ii) x−1/2, y+1/2, z−1/2; (iii) x+1/2, y−1/2, z−1/2; (iv) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | Pb5Al3F19 |
Mr | 1477.94 |
Crystal system, space group | Triclinic, I1 |
Temperature (K) | 320 |
a, b, c (Å) | 14.2624 (2), 14.2808 (2), 7.2340 (1) |
α, β, γ (°) | 90.001 (10), 90.509 (1), 90.001 (10) |
V (Å3) | 1473.39 (4) |
Z | 4 |
Radiation type | ?, λ = ? Å |
Specimen shape, size (mm) | ?, ? × ? × ? |
Data collection | |
Diffractometer | ? |
Specimen mounting | ? |
Data collection mode | ? |
Scan method | ? |
2θ values (°) | 2θmin = ? 2θmax = ? 2θstep = ? |
Refinement | |
R factors and goodness of fit | Rp = 0.078, Rwp = 0.112, Rexp = 0.049, χ2 = 5.290 |
No. of data points | ? |
No. of parameters | 146 |